• Title/Summary/Keyword: GC/NPD

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Development of Analytical Method for Fenoxanil in Agricultural Products Using GC-NPD and GC/MS (농산물 중 Fenoxanil 잔류성 시험법 개발)

  • Kim, Gyeong-Ha;Ahn, Kyung-Geun;Kim, Gi-Ppeum;Hwang, Young-Sun;Lee, Young Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.19 no.4
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    • pp.345-353
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    • 2015
  • The aim of this study is to develop residue analysis method for fenoxanil, a MBI (melanin biosynthesis inhibitor) propionamide fungicide, had mainly been used to control rice blast, and disease of other crops, fruits, and vegetables by using GLC/NPD and GC/MS. Extraction with acetone and partition with n-hexane/dichloromethane (80/20, v/v) were performed from hulled rice, soybean, Kimchi cabbage, green pepper, and apple, then column clean-up with florisil was applied. Mean recoveries were 82.2%-109.1% with less than 7.2% of coefficients of variation and limit of quantitation was set at the concentration of 0.04 mg/kg from the five agricultural products through the determination by GLC/NPD equipped with DB-5 capillary column and single laboratory validation. As a confirmatory method, GC/MS selected ion monitoring (SIM) was set from m/z 125.0, 188.9, and 293.0. Developed method is expected to apply the single residue analysis of fenoxanil in agricultural products.

Analysis of Multiple Pesticide Residues in Raw Materials Used in Dietary Supplements by GC/ECD and NPD (GC/ECD와 NPD를 이용한 건강기능식품 주요 원료 중 다성분 잔류농약 분석)

  • Park, Sun-Young;Oh, Sang-Suk
    • Korean Journal of Food Science and Technology
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    • v.36 no.6
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    • pp.863-871
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    • 2004
  • Analyses of residual pesticides in raw materials used for dietary supplements were performed using multi-ingredients simultaneous analysis method. Pesticides such as BHC, chlorpyrifos, and quintozene were detected in 12 domestic and 7 imported samples, suggesting need for monitoring pesticides in domestic and imported raw materials and establishing residual limit of each pesticide.

Monitoring of Uniconazole by GC-NPD (GC-NPD 동시분석법을 이용한 유니코나졸 잔류실태조사)

  • Kim, Eun-Jeung;Choi, Bu-Chuhl;Choi, Su-Jeong;Hong, Chae-Kyu;Kim, Eun-Hee;Choi, Chae-Man;Seo, Young-Ho;Hwang, Young-Sook;Jang, Mi-Ra;Hwang, In-Sook;Kim, Moo-Sang;Chae, Young-Zoo
    • Korean Journal of Food Science and Technology
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    • v.44 no.3
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    • pp.378-381
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    • 2012
  • The monitoring of the uniconazole residual pesticide for agricultural products was conducted by multiclass pesticide multiresidue methods. Samples were collected from June to November, 2011. Uniconazole pesticide was detected in 49 samples from a total of 3,939 samples. The amount of uniconazole pesticide ranged from 0.09 to 17.89 mg/kg in 49 samples. This method was described for the simultaneous determination of uniconazole by gas chromatography with a nitrogen phosphorus detector (GC-NPD) and mass spectrometry (MS). The limit of detection and quantification were 0.006 and 0.018 mg/kg GC-NPD, respectively. For an evaluation of the GC-NPD method, uniconazole spiked into gyeojachae at a level of 0.5, 5 mg/kg was determined. The recoveries of uniconazole by the GC-NPD method ranged from 83.4 to 101.4%. The results indicate that the method of simultaneous analysis is applicable to uniconazole analysis.

Evaluation of QuEChERS Method for Determination of pesticide Residues Using GC/NPD and GC/ECD (GC/NPD와 GC/ECD를 이용한 잔류농약 정량 분석법으로써의 QuEChERS의 평가)

  • Cho, Tae Hee;Park, Young Hye;Park, Hye Won;Hwang, Lae Hwong;Cho, In Soon;Kim, Min Jung;Kim, Hyun Jeong;Kim, Mu Sang;Chae, Young Zoo
    • The Korean Journal of Pesticide Science
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    • v.17 no.1
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    • pp.65-71
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    • 2013
  • The modified QuEChERS method was evaluated for rapid determination of pesticide residues in spinach by gas chromatography-nitrogen phosphorous detector (NPD) and electron capture detector (ECD). Fifty GC-amenable pesticides which were most frequently detected in monitoring were selected in the current study. Matrix-matched calibration was performed. The detector response for all pesticides was linear with determination coefficients higher than 0.995. LODs for most compounds ranged between 0.001 and 0.1 ug/g, and about 90% of the compounds had LODs of less than 0.05 ug/g. LOQs ranged from 0.001 to 0.32 ug/g, which were well below the MRLs permitted for most of pesticides. In the majority of cases, the recoveries (80-120%) and relative standard deviations (RSDs) (less than 20%) were within acceptable levels except for dichlorvos, propamocarb, chlorothalonil, dichlofluanid, cyhalothrin and fenvalerate. Also, this method which is applied to routine samples showed good results when comparing with traditional multi-residue method.

Modified QuEChERS Multi-Residue Analysis Method for 61 pesticides in Fruits using with HPLC and GC-ECD/NPD (HPLC 및 GC-ECD/NPD를 이용한 과일 중 61종 농약의 QuEChERS 전처리 다성분 분석법 개발)

  • Lee, Ju-Young;Hong, Su-Myeong;Kim, Taek-Kyum;Min, Zaw Win;Kim, Yang-Hyeon;Song, Kyung-Ae;Kwon, Hye-Yong;Lee, Hee-Dong;Im, Geon-Jae;Kim, Doo-Ho;Kim, Jang-Eok
    • The Korean Journal of Pesticide Science
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    • v.16 no.3
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    • pp.242-256
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    • 2012
  • QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method has been a lot of research for pesticide analysis, because it is very simple and fast. However, this method requires high sensitivity instrument such as LC-MS/MS because of the use of small sample volume and many impurities compared to the conventional method. So, QuEChERS method needs to be modified for using with HPLC and GC-ECD/NPD. The aim of this work was to study the application of the QuEChERS method as well as its modification for the extraction and preconcentration of 5 groups of 61 pesticides from 4 fruits prior to their determination by HPLC-PDA, GC-ECD/NPD, and LC-MS/MS. The method was validated using spiking levels at 0.1 mg/kg (or 0.01 mg/kg) in apple, grapes, pear and persimmon. The average recovery by QuEChERS AOAC Official 2007. 01 version using the LC-MS/MS varied from 71.1127.4% for 61 pesticides. The average recovery rates using modified QuEChERS varied from 70.9~126% for 61 pesticides by HPLC-PDA and GC-ECD/NPD. The results satisfied the criteria of multiple pesticide residue analysis, setting 70~130% for recovery rates and below 30% for CV.

Determination of residual pesticides in crude drugs - Gas chromatographic Analysis of 18 pesticides - (한약재중의 잔류농약 분석 - GC에 의한 18종 잔류농약의 분석 -)

  • Hwang, In-Sook;Choi, Byung-Hyun;Bae, Chong-Ho;Kim, Myung-Hee;Cho, Hae-Jeon
    • Korean Journal of Pharmacognosy
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    • v.32 no.3 s.126
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    • pp.200-211
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    • 2001
  • This study was carried out to determine the 11 organochlorine, 7 organophosphorus residual pesticides in 251 crude drugs. These residual pesticides in herbal drugs were extracted with acetonitrile and the extracts were cleaned up via LC-florisil solid phase extraction column. The prepared samples were assayed for pesticide residues using GC-ECD, NPD with capillary column and identified by GC-MSD. Recoveries were $63.9{\sim}111.5%$ in the organochlorine pesticides and $69.8{\sim}92.4%$ in the organophosphorus pesticides, and detection limits were $0.001{\sim}0.65\;ppm$ in the organochlorine pesticides and $0.0009{\sim}0.0074\;ppm$ in the organophosphorus pesticides. Pesticide residues were detected in 9 cases.

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Distributions of Nicotine and Toluene in Teenagers' Urine (청소년의 뇨 중에서 nicotine과 톨루엔의 분포에 관한 연구)

  • Park, Sungwoo;Seo, Baeseck;You, Jaehoon;Kim, Namyee;Shin, Hosang;Han, Wansoo;Kim, Ilkwang
    • Analytical Science and Technology
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    • v.10 no.1
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    • pp.1-8
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    • 1997
  • We identified nicotine, cotinine and toluene in high school volunteer's urine by using GC/NPD, GC/FID and GC/MS. To analyze of nicotine and cotinine, urine samples were extracted with diethylether and centrifuged on a benchtop centrifuge for 5 min. The upper organic layer was injected into a GC. The distributions of nicotine and cotinine were $4{\sim}630{\mu}g/L$ and $63{\sim}1,602{\mu}g/L$ in smoking-group, respectively. To analyze of toluene, head space vial was filled with 2mL sodium citrate solution and 1mL of urine. The vial was warmed in a water bath at $55^{\circ}C$ for 20min, and then $250{\mu}L$ of head space air was injected into a GC. The result show that toluene was not detected in all of the volunteers' samples. However, the range of toluene was 0.1~28.0mg/L in glue sniffer's urine samples(NISI data).

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Simultaneous Determination of Simetryn and Buprofezin by Gas Chromatography with Nitrogen Fhosphorus Detector (GC-NPD를 이용한 Simetryn과 Buprofezin의 동시 분석법 연구)

  • Kim Eunjeung;Kim Sungdan;Lee Jaekyoo;Kim Soojin;Lee Sangmi;Han Sunhee;Kang Heegon
    • Journal of Food Hygiene and Safety
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    • v.20 no.3
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    • pp.159-164
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    • 2005
  • This method was described for the simultaneous determination of simetryn and buprofezin in rice, vegetables, and fruits by gas chromatography(GC) with nitrogen phosphorus detector. The GC method of simetryn and buprofezin was shown to give a linear detection ranges between $0.019\sim9.306mg/kg,\;0.023\sim11.27mg/kg$, respectively. For evaluation of GC method, simetryn spiked into rice, vegetables and fruits at the level of 4.653mg/kg was determined. The recoveries of simetryn by GC method were ranged from 57.9 to $115.9\%$. For evaluation of GC method, buprofezin spiked into rice, vegetables and fruits at the level of 2.817mg/kg was determined. The recoveries of buprofezin by GC method were ranged from 56.5 to $121.5\%.$